CN103198928B - A kind of sodium ion electrochemical capacitor - Google Patents
A kind of sodium ion electrochemical capacitor Download PDFInfo
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- CN103198928B CN103198928B CN201210004771.9A CN201210004771A CN103198928B CN 103198928 B CN103198928 B CN 103198928B CN 201210004771 A CN201210004771 A CN 201210004771A CN 103198928 B CN103198928 B CN 103198928B
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Abstract
The invention provides a kind of sodium ion electrochemical capacitor, including: positive pole, negative pole, electrolyte and the barrier film between both positive and negative polarity, the material of described sodium ion electrochemical capacitor negative pole is coke, molybdenum sulfide, molybdenum oxide, niobium oxide or sodium titanate, and described electrolyte is the organic solution of neutral sodium-salt.Described five kinds of negative materials are layer structure, therefore the sodium ion in electrolyte can embed on negative material surface and deviate from, namely there is redox reaction, and the interlamellar spacing of negative material is bigger, it is more beneficial for larger-size sodium ion quickly embed and deviate from, thus improving the energy density of sodium ion electrochemical capacitor, power density and cycle life.The sodium ion electrochemical capacitor negative material of the present invention adopts coke, molybdenum sulfide, molybdenum oxide, niobium oxide or sodium titanate simultaneously, and electrolyte is the organic solution of neutral sodium-salt, effectively reduces the cost of capacitor.
Description
Technical field
The present invention relates to capacitor area, particularly relate to a kind of sodium ion electrochemical capacitor.
Background technology
Electrochemical capacitor is also known as ultracapacitor, ultracapacitor is made up of positive pole, negative pole, electrolyte and the barrier film between both positive and negative polarity, it is a kind of novel electrochemical energy storage and conversion equipment, has higher faraday's specific capacitance and energy density compared with common capacitor；Then there is power density height compared with accumulator, the discharge and recharge time is short, cyclicity good, long service life and be easy to safeguard feature.Electrochemical capacitor has the dual-use function of traditional capacitor and battery, and its power density is far above common batteries, and energy density is far above traditional capacitance, thus has filled up the blank of the two conventional art.
Electrochemical capacitor is built upon the novel energy-storing device on electrochemical principle basis.Rise and development along with environmental-protecting type electric automotive research, in the dynamical system of the electric automobile designed and developed and composite electric automobile, if being used alone battery to will be unable to meet the requirement of dynamical system, but hybrid power source system high power density electrochemical capacitor and high energy density cells composed in parallel both had met the needs of high power density, met again the needs of high-energy-density.High-energy-density, high power density electrochemistry electrical equipment become people research focus.Current electrochemical capacitor is widely used; such as: electrochemical capacitor and all kinds of electrokinetic cells are with the use of composition composite battery; it is applied to the power initiation system of electric automobile, the starting of vehicle, acceleration and braking procedure play protection accumulator and energy-conservation effect.Electrochemical capacitor can directly as the power supply of electric motor car, it is also possible to for the big electric current that the startup system offer of internal combustion engine and other engine of heavy-duty cars is instantaneous.
The maximum advantage of electrochemical capacitor is in that it has higher power density, namely excellent fast charging and discharging performance；The energy density that its shortcoming is electrochemical capacitor is relatively low relative to lithium battery.In order to improve energy density, researcher proposes the concept mixing type electrochemical capacitor, namely an electrode of capacitor uses the material with carbon element of double layer capacitor, and another electrode uses battery material, and this battery material mainly occurs the lithium of faraday's reaction to embed complex.Lithium embeds the introducing of complex and this kind of energy density mixing type capacitor is greatly improved.The material of this kind of capacitor is mainly lithium complex, and its electrolyte is also mainly lithium salts, and therefore this kind of type capacitor that mixes is also known as lithium ion hydridization capacitor.But lithium is as minor metals a kind of in nature, its content is limited, so the cost of this kind of capacitor is significantly high.
Summary of the invention
Present invention solves the technical problem that the sodium ion electrochemical capacitor being in that to provide a kind of low cost, sodium ion electrochemical capacitor provided by the invention has higher power density and energy density and good cycle life simultaneously.
The invention provides a kind of sodium ion electrochemical capacitor, including: positive pole, negative pole, electrolyte and the barrier film between both positive and negative polarity, the material of described negative pole is coke, molybdenum sulfide, molybdenum oxide, niobium oxide or sodium titanate, and described electrolyte is the organic solution of neutral sodium-salt.
Preferably, the material of described negative pole is molybdenum oxide or sodium titanate.
Preferably, the material of described negative pole is molybdenum oxide nano belt or sodium titanate nanotubes.
Preferably, the preparation method of described sodium titanate nanotubes is: be dissolved in sodium hydroxide solution by titanium-containing compound and tetrabutyl titanate ester, at 130 DEG C～180 DEG C hydro-thermal 36h～72h, product is sequentially carried out washing and calcines at 300 DEG C～600 DEG C after drying；Described titanium-containing compound is titanium dioxide, titanyl sulfate or titanium tetrachloride.
Preferably, described titanium-containing compound is titanium dioxide.
Preferably, described concentration of electrolyte is 1～1.5M.
Preferably, described neutral sodium-salt is sodium tetrafluoroborate, sodium hexafluoro phosphate or sodium perchlorate.
Preferably, described neutral salt is sodium perchlorate.
Preferably, the organic solvent of described electrolyte is one or both in Allyl carbonate, ethylene carbonate, diethyl carbonate and dimethyl carbonate.
Preferably, described just extremely active carbon electrode or graphite electrode.
Compared with prior art, the negative material that the present invention adopts is coke, molybdenum sulfide, molybdenum oxide, niobium oxide or sodium titanate, and electrolyte is the organic solution of neutral sodium-salt, effectively reduces the cost of electrochemical capacitor.Negative material in the present invention selects coke, molybdenum sulfide, molybdenum oxide, niobium oxide or sodium titanate, these five kinds of negative materials are all layer structures, when charging, larger-size sodium ion is embedded in the negative material of layer structure, so that substantial amounts of electric charge stores in the electrodes, and these sodium ion entering negative material can come back in electrolyte when electric discharge, the electric charge simultaneously stored is discharged by external circuit, the process of discharge and recharge is the course of reaction that sodium ion embeds at negative material and deviates from, and negative material has bigger interlamellar spacing, it is more beneficial for larger-size sodium ion quickly embed at interlayer and deviate from, coordinate again and adopt the neutral sodium-salt that dissolubility in the electrolytic solution is bigger, thus being conducive to sodium ion electrochemical capacitor to have higher energy density and power density.Meanwhile, only there is the embedding of ion and deviate from sodium ion electrochemical capacitor in charge and discharge process, it does not have other chemical reaction occurs, and electrode structure does not change, and therefore sodium ion electrochemical capacitor has good cycle life.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the sodium titanate nanotubes do not calcined of the embodiment of the present invention 2 preparation；
Fig. 2 is the transmission electron microscope picture of the sodium titanate nanotubes do not calcined of the embodiment of the present invention 2 preparation；
Fig. 3 is the transmission electron microscope picture of the sodium titanate nanotubes of 300 DEG C of calcinings of the embodiment of the present invention 2 preparation；
Fig. 4 is the transmission electron microscope picture of the sodium titanate nanotubes of 400 DEG C of calcinings of the embodiment of the present invention 2 preparation；
Fig. 5 is the transmission electron microscope picture of the sodium titanate nanotubes of 500 DEG C of calcinings of the embodiment of the present invention 2 preparation；
Fig. 6 is the transmission electron microscope picture of the sodium titanate nanotubes of 600 DEG C of calcinings of the embodiment of the present invention 2 preparation；
Fig. 7 is the X-ray diffractogram of the sodium titanate nanotubes of the embodiment of the present invention 2 preparation；
Fig. 8 is the specific capacitance of single electrode curve chart of the sodium titanate of the embodiment of the present invention 3 preparation；
Fig. 9 is the specific capacitance of single electrode curve chart of the molybdenum sulfide of the embodiment of the present invention 3 preparation, molybdenum oxide and tungsten oxide；
Figure 10 is the specific capacitance of single electrode curve chart of the niobium oxide of the embodiment of the present invention 3 preparation；
Figure 11 is the sodium titanate specific capacity curve chart with the full battery of activated carbon different quality proportioning assembling of the embodiment of the present invention 4 preparation；
Figure 12 is the asymmetric capacitor of sodium ion of the embodiment of the present invention 5 preparation and the energy density of activated carbon/activated carbon symmetric capacitor and power density curve chart；
Figure 13 is the asymmetric capacitor cycle charging and discharging curve figure of sodium ion of the embodiment of the present invention 6 preparation.
Detailed description of the invention
In order to be further appreciated by the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but it is to be understood that these describe simply as further illustrating the features and advantages of the present invention, rather than limiting to the claimed invention.
The embodiment of the invention discloses a kind of sodium ion electrochemical capacitor, including: positive pole, negative pole, electrolyte and the barrier film between both positive and negative polarity, the material of described negative pole is coke, molybdenum sulfide, molybdenum oxide, niobium oxide or sodium titanate, and described electrolyte is the organic solution of neutral sodium-salt.
According to the present invention, the negative material of described sodium ion electrochemical capacitor is coke, molybdenum sulfide, molybdenum oxide, niobium oxide or sodium titanate, in order to obtain power density and the higher sodium ion electrochemical capacitor of energy density, molybdenum oxide in negative material of the present invention is preferably molybdenum oxide nano belt, and sodium titanate is preferably sodium titanate nanotubes.
Described sodium titanate nanotubes can be prepared as follows: is dissolved in sodium hydroxide solution by titanium-containing compound and tetrabutyl titanate ester, at 130 DEG C～180 DEG C hydro-thermal 36h～72h, product is sequentially carried out washing and calcines at 300 DEG C～600 DEG C after drying；Described titanium-containing compound is titanium dioxide, titanyl sulfate or titanium tetrachloride.
Due to the negative material coke that the present invention adopts, molybdenum oxide, niobium oxide, molybdenum sulfide and sodium titanate are all layer structures, when charging, larger-size sodium ion is embedded in the negative material lattice of layer structure, so that substantial amounts of electric charge stores in the electrodes, and these sodium ion entering negative material can come back in electrolyte when electric discharge, the electric charge simultaneously stored is discharged by external circuit, the process of discharge and recharge is the course of reaction that sodium ion embeds at negative material and deviates from, the interlamellar spacing of negative material is more beneficial for more greatly quickly embedding and deviating from of sodium ion simultaneously, so that high rate performance is greatly improved, namely power density and energy density are improved.
In order to improve the performance of electrochemical capacitor, in addition it is also necessary to the electrolyte of electrochemical capacitor is carried out considered critical.Electrolyte in the present invention is the organic solution of neutral sodium-salt, described neutral sodium-salt is preferably sodium tetrafluoroborate, sodium hexafluoro phosphate or sodium perchlorate, it is more preferably sodium perchlorate, these three neutral sodium-salt has bigger dissolubility in organic solution, and it is more stable, therefore the sodium ion existed in the electrolytic solution is more, it is possible to for providing more free ion in electrolyte.
The organic solution of the present invention is preferably one or both in Allyl carbonate, ethylene carbonate, diethyl carbonate and dimethyl carbonate, described organic solvent has relatively low viscosity, ensure that sodium ion has quick migration velocity, and described organic solvent has moderate conductivity and wider electrochemical window, thus being conducive to improving energy density and the power density of electrochemical capacitor.The concentration of electrolyte of the present invention is preferably 1～1.5M, if because the viscosity that salinity too conference causes electrolyte increases, is unfavorable for that sodium ion fast transferring deviates from reaction to electrode surface generation embedding, thus reducing energy density and the power density of electrochemical capacitor.
The negative material of the electrochemical capacitor of the present invention is coke, molybdenum sulfide, molybdenum oxide, niobium oxide or sodium titanate, and electrolyte is the organic solution of neutral sodium-salt, advantageously reduces the cost of electrochemical capacitor.Negative material in the electrochemical capacitor of the present invention is all layer structure simultaneously, and interlamellar spacing is bigger, it is thus advantageous to larger-size sodium ion quickly embed at interlayer and deviate from, there is redox reaction, and coordinate the neutral sodium-salt adopting dissolubility in the electrolytic solution bigger, thus be conducive to improving sodium ion electrochemical capacitor energy density, power density.Only there is the embedding of ion and deviate from sodium ion electrochemical capacitor, it does not have other chemical reaction occurs in charge and discharge process, and electrode structure does not change, and therefore sodium ion electrochemical capacitor has good cycle life.
In order to be further appreciated by the present invention, below in conjunction with embodiment, sodium ion electrochemical capacitor provided by the invention being described in detail, protection scope of the present invention is not limited by the following examples.
Embodiment 1
It is dissolved in 40ml distilled water by 0.4g sodium molybdate ultrasonic 0.5h, is injected in 50ml stainless steel cauldron after regulating pH to 1.2 with 1MHCl and 1MNaOH, after 160 DEG C of hydro-thermal 24h, naturally cools to room temperature.Then repeat 3 times with distilled water wash is centrifugal, repeat 3 times with absolute ethanol washing is centrifugal, last 60 DEG C of vacuum drying 10h, obtain molybdenum oxide nano belt.
Molybdenum oxide in following example is prepared by embodiment 1.
Embodiment 2
Being dissolved in the sodium hydroxide solution of 80 milliliters of 10M by titanium dioxide commercially available for 1g and tetrabutyl titanate ester respectively, stirring proceeded in 100 milliliters of reactors after 3 hours at room temperature, 150 DEG C of hydro-thermal 48h.Hydro-thermal after terminating to be down to room temperature product proceeded to 1000 milliliters of secondary water wash to pH be 7～8.60 DEG C of dried calcining 5h in the high temperature of 300 DEG C, 400 DEG C, 500 DEG C and 600 DEG C respectively.The sodium titanate nanotubes do not calcined is labeled as T0, the sodium titanate nanotubes of 300 DEG C of calcinings is labeled as T1, the sodium titanate nanotubes of 400 DEG C of calcinings is labeled as T2, the sodium titanate nanotubes of 500 DEG C of calcinings is labeled as T3, the sodium titanate nanotubes of 600 DEG C of calcinings is labeled as T4。
Adopting RigakuD/max-IIB type diffractometer, Cu target K alpha ray makes X-ray source, and sweep limits is 5 °～60 °, and scanning speed is 1 °/min.Comparison PDF data card, obtains the X-ray diffractogram of sodium titanate.In Fig. 1, curve a～e is followed successively by T0、T1、T2、T3And T4X-ray diffractogram, in Fig. 1, zero place represents Na2Ti6O13Diffraction maximum, * place represents Na2Ti3O7Diffraction maximum, feature XRD diffraction maximum prove sodium titanate nanotubes can successfully prepare.
The XL-30ESEM type scanning electron microscope adopting PHILIPS Co. is used for characterizing pattern and the composition of sodium titanate nanotubes, and accelerating potential is 15kV.Fig. 2 is T0Scanning electron microscope (SEM) photograph, Fig. 3 is T0Transmission electron microscope picture, sodium titanate is length hollow sodium mitron between hundreds of nanometers to micron as shown in Figure 3, between caliber about 6～10 microns.Fig. 4～Fig. 7 is T respectively1、T2、T3And T4Transmission electron microscope picture.As seen from the figure, after high-temperature calcination, the pattern of sodium titanate changes, T1～T3It is hollow nanotube-shaped, T4Pattern becomes either solid nanorods.
In following example, sodium titanate is prepared by embodiment 2.
Embodiment 3
Respectively by 6mgT1～T4, coke, molybdenum sulfide, molybdenum oxide and niobium oxide and the mixing of 3mg electroconductive binder be coated in the online tabletting film forming of rustless steel battery current collecting, proceed in the glove box that anhydrous and oxygen-free argon is saturated at 180 DEG C of vacuum dryings after 3 hours, respectively with T1～T4, coke, molybdenum sulfide, molybdenum oxide and niobium oxide be positive pole, metallic sodium is negative pole, and the organic solution of 1.5M sodium perchlorate is electrolyte, and a polyethylene film and a glass fibre are barrier film, it is assembled into button cell, under the running voltage of 0.1～2.5V, makes charge-discharge test.
Fig. 8 is sodium titanate single electrode charging and discharging capacity curve chart, and in Fig. 8, ■ curve is T1Single electrode charging and discharging capacity curve, ● curve is T2Single electrode charging and discharging capacity curve, ▲ curve is T3Single electrode charging and discharging capacity curve, curve is T4Single electrode charging and discharging capacity curve.
Fig. 9 is the single electrode charging and discharging capacity curve chart of molybdenum sulfide, molybdenum trioxide, tungsten oxide and molybdenum dioxide, in Fig. 9, ■ curve is the single electrode charging and discharging capacity curve of molybdenum sulfide, ● curve is the single electrode charging and discharging capacity curve of molybdenum trioxide, ▲ curve is the single electrode charging and discharging capacity curve of tungsten oxide, and curve is the single electrode charging and discharging capacity curve of molybdenum dioxide.Figure 10 is the single electrode charging and discharging capacity curve chart of niobium oxide.
Embodiment 4
T by different quality proportioning2Help battery with activated carbon assembling and carry out charge-discharge test, T2It is 1: 8,1: 6,1: 4,1: 2,1: 1.5 and 1: 1 with the mass ratio of activated carbon.Figure 11 is T2Specific capacity curve chart with the full battery that activated carbon different quality proportioning assembles.In Figure 11, ■ curve is T2The charging and discharging capacity curve of the full battery assembled when being 1: 1 with quality of activated carbon ratio, ● curve is T2The charging and discharging capacity curve of the full battery assembled when being 1: 1.5 with quality of activated carbon ratio, ▲ curve is T2The charging and discharging capacity curve of the full battery assembled when being 1: 2 with quality of activated carbon ratio, ◆ curve is T2The charging and discharging capacity curve of the full battery assembled when being 1: 4 with quality of activated carbon ratio, curve is T2The charging and discharging capacity curve of the full battery assembled when being 1: 6 with quality of activated carbon ratio,Curve is T2The charging and discharging capacity curve of the full battery assembled when being 1: 8 with quality of activated carbon ratio.
Embodiment 5
With T2For negative pole, activated carbon is positive pole, it is assembled into asymmetric capacitor, simultaneously in order to contrast, activated carbon does both positive and negative polarity respectively, it is assembled into symmetric capacitor, the organic solution of 1.5M sodium perchlorate is electrolyte, one polyethylene film and a glass fibre are barrier film, it is assembled into button cell, asymmetric capacitor makes charge-discharge test under the running voltage of 0～3V, adopt LAND series battery test system respectively at 1mA, 2mA, 3mA, 4mA, 5mA, 6mA, 7mA, 8mA, 9mA, charge-discharge test is carried out under 10mA electric current density, obtain curve chart as shown in figure 12, Figure 12 is power density and the energy density profile figure of the asymmetric capacitor of sodium ion and activated carbon/activated carbon symmetric capacitor.In Figure 12 ● curve is T2With the power density of the asymmetric capacitor of activated carbon assembling and energy density profile, ■ curve is power density and the energy density profile of the symmetric capacitor that activated carbon assembles with activated carbon.As shown in Figure 12, the symmetric capacitor that the asymmetric capacitor specific activity charcoal that sodium titanate and activated carbon assemble and activated carbon assemble has higher energy density and power density.
Embodiment 6
With T2For negative pole, activated carbon is positive pole, the organic solution of 1.5M sodium perchlorate is electrolyte, one polyethylene film and a glass fibre are barrier film, it is assembled into button cell, discharge and recharge 1000 times under the running voltage and 1mA electric current density of 0-3V, Figure 13 is the cycle charge-discharge curve of the button cell assembled, in figure, solid dot represents electric discharge, and hollow dots represents charging.In Figure 13, solid dot and hollow dots essentially coincide, it follows that the capability retention that the asymmetric capacitor of sodium ion is in 1000 charge and discharge process is higher, illustrate that cycle life is better.
The explanation of above example is only intended to help to understand method and the core concept thereof of the present invention.It should be pointed out that, for those skilled in the art, under the premise without departing from the principles of the invention, it is also possible to the present invention carries out some improvement and modification, these improve and modify in the protection domain also falling into the claims in the present invention.
Described above to the disclosed embodiments, makes professional and technical personnel in the field be capable of or uses the present invention.The multiple amendment of these embodiments be will be apparent from for those skilled in the art, and generic principles defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention is not intended to be limited to the embodiments shown herein, and is to fit to the widest scope consistent with principles disclosed herein and features of novelty.
Claims (7)
1. a sodium ion electrochemical capacitor, including: positive pole, negative pole, electrolyte and the barrier film between both positive and negative polarity；It is characterized in that, the material of described negative pole is sodium titanate, described electrolyte is the organic solution of neutral sodium-salt, and the organic solvent of described electrolyte is one or both in Allyl carbonate, ethylene carbonate, diethyl carbonate and dimethyl carbonate, described just extremely activated carbon electrodes or graphite electrode.
2. sodium ion electrochemical capacitor according to claim 1, it is characterised in that the material of described negative pole is sodium titanate nanotubes.
3. sodium ion electrochemical capacitor according to claim 2, it is characterised in that the preparation method of described sodium titanate nanotubes is:
Titanium-containing compound and tetrabutyl titanate ester are dissolved in sodium hydroxide solution, at 130 DEG C～180 DEG C hydro-thermal 36h～72h, product are sequentially carried out washing and calcine at 300 DEG C～600 DEG C after drying；Described titanium-containing compound is titanium dioxide, titanyl sulfate or titanium tetrachloride.
4. sodium ion electrochemical capacitor according to claim 3, it is characterised in that described titanium-containing compound is titanium dioxide.
5. sodium ion electrochemical capacitor according to claim 1, it is characterised in that described concentration of electrolyte is 1～1.5M.
6. sodium ion electrochemical capacitor according to claim 1, it is characterised in that described neutral sodium-salt is sodium tetrafluoroborate, sodium hexafluoro phosphate or sodium perchlorate.
7. sodium ion electrochemical capacitor according to claim 6, it is characterised in that described neutral sodium-salt is sodium perchlorate.
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| CN102683039A (en) * | 2012-05-15 | 2012-09-19 | 中国科学院长春应用化学研究所 | Electrochemical capacitor |
| CN104091915B (en) * | 2014-07-17 | 2016-07-06 | 浙江大学 | The electrochemistry storage sodium combination electrode of a kind of high power capacity and stable circulation and preparation method |
| US10102982B2 (en) | 2015-03-03 | 2018-10-16 | Ut-Battelle Llc | Electrolytes for supercapacitors |
| CN104966621B (en) * | 2015-05-14 | 2018-10-02 | 中国科学院青岛生物能源与过程研究所 | A kind of solvent is total to embedded type sodium ion capacitor |
| CN108242543A (en) * | 2016-12-26 | 2018-07-03 | 福建新峰二维材料科技有限公司 | A kind of soft carbon makees the preparation method of the sodium Dual-ion cell of negative material |
| CN107369560B (en) * | 2017-08-04 | 2019-02-19 | 哈尔滨工业大学 | A kind of flexibility sodium ion capacitor and preparation method thereof |
| CN108630441B (en) * | 2018-04-28 | 2020-09-04 | 南京林业大学 | Biomass hierarchical porous carbon loaded nano-structure sodium titanate and preparation method thereof |
| CN110165303B (en) * | 2019-06-10 | 2022-04-26 | 南京理工大学北方研究院 | Secondary battery, preparation method thereof and electric equipment |
| CN112542326B (en) * | 2020-04-29 | 2022-02-08 | 华中科技大学 | Universal method for improving performance of layered electrode material by regulating and controlling electrolyte composition |
| CN116282168A (en) * | 2023-03-16 | 2023-06-23 | 广州大学 | Lithium ion battery negative electrode material, and preparation method and application thereof |
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| JP5375580B2 (en) * | 2008-12-18 | 2013-12-25 | 株式会社エクォス・リサーチ | Electrolyte for sodium ion battery |
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